反応 #1791507
ord-43af29c1327347f688da3bc820bab4dc
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.ADDITIONAfter the addition
- 2ろ過was filtered
- 3workup.ADDITIONA drop of concentrated hydrochloric acid was added to the filtrate which
- 4その他removed some color
- 5その他to yield a cream color material
- 6その他Recrystallization from toluene
- 7その他gave needles, (93% yield)
- 8その他sintered at 177° C.
実験手順
A stirred solution of 9 g. (0.028 mole) of 7-(4-chlorobenzoyl)-3-methylthioindolin-2-one in 180 ml. of tetrahydrofuran was treated over a two-hour period with 45 g. of a commercial Raney nickel water suspension. After the addition was complete the mixture was filtered. A drop of concentrated hydrochloric acid was added to the filtrate which removed some color and the resulting solution was then stripped under water pump vacuum to yield a cream color material. Recrystallization from toluene gave needles, (93% yield); the material sintered at 177° C. and melted at 186° C.